CN114855020A - Preparation process of oxygen-free copper-based high-strength composite material - Google Patents
Preparation process of oxygen-free copper-based high-strength composite material Download PDFInfo
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- CN114855020A CN114855020A CN202210538744.3A CN202210538744A CN114855020A CN 114855020 A CN114855020 A CN 114855020A CN 202210538744 A CN202210538744 A CN 202210538744A CN 114855020 A CN114855020 A CN 114855020A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 71
- 239000010949 copper Substances 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000000843 powder Substances 0.000 claims abstract description 38
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 30
- 238000005245 sintering Methods 0.000 claims abstract description 30
- 239000002245 particle Substances 0.000 claims abstract description 25
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 24
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 25
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 23
- 239000010439 graphite Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 17
- 239000011812 mixed powder Substances 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 13
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 13
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 10
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 238000002490 spark plasma sintering Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 2
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000002708 enhancing effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000005728 strengthening Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 229910000881 Cu alloy Inorganic materials 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0084—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ carbon or graphite as the main non-metallic constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses a preparation process of an oxygen-free copper-based high-strength composite material, which comprises the steps of uniformly mixing chromium powder, nano titanium carbide and a graphene/copper composite powder according to the formula amount to obtain a mixture, placing the mixture in a mold, carrying out discharge plasma sintering under protective gas, wherein the sintering temperature is 850-, the copper particles keep fine size, which is beneficial to enhancing the mechanical property of the oxygen-free copper-based high-strength composite material.
Description
Technical Field
The invention relates to the technical field of oxygen-free copper-based materials, in particular to a preparation process of an oxygen-free copper-based high-strength composite material.
Background
With the continuous development of information technology, the microelectronic industry has higher and higher requirements for conductive metal materials, and the trend of the requirements is that the conductive metal materials have high conductivity, high strength and high temperature resistance, copper and copper alloys are frequently used in the industry for a long time, and more than 75% of copper and copper alloys are used in the electrical and electronic industries. Pure copper has excellent electrical and thermal conductivity, but its obvious disadvantages are its low hardness, tensile strength and creep strength, such as its strength is 230 MPa-290 MPa, and after cold deformation, its strength can reach 400MPa, but its elongation is only 2%, and it is lost quickly in the tempering process.
The composite strengthening mode of introducing proper strengthening phase(s) can not only play the synergistic effect of the matrix and the strengthening material, but also has great design freedom, but also can not give consideration to the strength and the conductivity of the composite material because the compatibility between the strengthening material and the copper-based raw material is poor when the strengthening material is directly added.
Disclosure of Invention
The invention aims to provide a preparation process of an oxygen-free copper-based high-strength composite material, which comprises the steps of uniformly mixing chromium powder, nano titanium carbide and graphene/copper composite powder according to the formula amount to obtain a mixture; placing the obtained mixture in a mold, performing discharge plasma sintering under protective gas, wherein the sintering temperature is 850-1000 ℃, the applied pressure is 20-50MPa, the sintering heat preservation time is 5-7min, and after natural cooling, demolding to obtain the oxygen-free copper-based high-strength composite material.
The purpose of the invention can be realized by the following technical scheme:
a preparation process of an oxygen-free copper-based high-strength composite material comprises the following steps:
the method comprises the following steps: uniformly mixing chromium powder, nano titanium carbide and graphene/copper composite powder according to the formula amount to obtain a mixture;
step two: and (3) placing the mixture obtained in the step one in a mold, performing discharge plasma sintering under protective gas, wherein the sintering temperature is 850-1000 ℃, the applied pressure is 20-50MPa, the sintering heat preservation time is 5-7min, and demolding after natural cooling to obtain the oxygen-free copper-based high-strength composite material.
As a further scheme of the invention: the preparation of the graphene/copper composite powder in the first step comprises the following steps:
the method comprises the following steps: adding copper acetate into ammonia water, and uniformly mixing to obtain a copper ammonia solution;
step two: adding graphite oxide sol into the copper ammonia solution obtained in the step one, and carrying out ultrasonic treatment for 35-45 minutes to obtain a mixed solution A;
step three: stirring the mixed solution A for 30 minutes at a speed of 200r/min by a magnetic stirrer, heating the mixed solution A to 100 ℃, and evaporating to dryness to obtain mixed powder;
step four: and continuously heating the mixed powder until the mixed powder is dried to obtain dry powder, and reducing the dry powder to obtain the graphene/copper composite powder.
As a further scheme of the invention: the mass ratio of the copper acetate to the ammonia water to the graphite oxide sol is 1:2: 1.
As a further scheme of the invention: the preparation of the graphite oxide sol is to disperse graphene oxide powder in water and obtain the graphite oxide sol through ultrasonic treatment.
As a further scheme of the invention: the heating temperature of the mixed powder in the fourth step is 240 ℃, and the continuous heating time is 6-8 hours.
As a further scheme of the invention: and in the fourth step, the dry powder is reduced by hydrogen, and the introduction rate of the hydrogen is 10 mL/min.
As a further scheme of the invention: the weight ratio of the chromium powder to the nano titanium carbide to the graphene/copper composite powder is 10-30: 1-5: 70-90.
As a further scheme of the invention: the chromium powder is prepared by ball milling raw material chromium powder with the particle size range of 50-200 mu m and the median particle size of 100 mu m;
the nano titanium carbide is prepared by ball milling raw material nano titanium carbide with the particle size range of 100-300 mu m and the median particle size of 120 mu m.
As a further scheme of the invention: and in the second step, the protective gas is argon.
As a further scheme of the invention: the temperature rise process of the spark plasma sintering in the second step is as follows: the sintering furnace chamber is vacuumized to 5Pa and then heated to 650 ℃ at the speed of 100 ℃/s, and after the temperature is kept for 5-7min, the temperature is raised to the sintering temperature of 850 ℃ and 1000 ℃ at the speed of 100 ℃/s.
The invention has the beneficial effects that:
(1) according to the invention, the graphene/copper composite powder is adopted, and the graphene has extremely high specific surface area, so that the relation between the graphene and a matrix is increased, more interfaces are generated, meanwhile, the graphene can effectively block the contact between the body material particles, a layer of film-shaped graphene is attached to the surface of the copper particles, the copper particles cannot grow up in the sintering process, the copper particles keep fine sizes, and the fine crystal grains can generate a fine grain strengthening effect, thereby being beneficial to enhancing the mechanical property of the oxygen-free copper-based high-strength composite material.
(2) The nano titanium carbide adopted by the invention has the characteristics of high hardness, high strength, high chemical stability, no hydrolysis and good high-temperature oxidation resistance, makes up for the defect of low strength and low hardness of the traditional copper material, improves the strength and the hardness of the material while ensuring the original corrosion resistance and machinability, and further prolongs the service life of the material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation process of an oxygen-free copper-based high-strength composite material comprises the following steps:
the method comprises the following steps: uniformly mixing chromium powder, nano titanium carbide and graphene/copper composite powder according to the formula amount to obtain a mixture;
wherein the mixture comprises the following raw materials in parts by weight: 10 parts of chromium powder, 1 part of nano titanium carbide and 70 parts of graphene/copper composite powder;
the graphene/copper composite powder comprises copper acetate, ammonia water and graphite oxide sol, wherein the mass ratio of the copper acetate to the ammonia water to the graphite oxide sol is 1:2: 1;
the chromium powder is prepared by ball milling raw material chromium powder with the particle size range of 50-200 mu m and the median particle size of 100 mu m; the nano titanium carbide is prepared by ball milling raw material nano titanium carbide with the particle size range of 100-300 mu m and the median particle size of 120 mu m;
step two: and (3) placing the mixture obtained in the step one in a mould, performing discharge plasma sintering in an argon environment, wherein the sintering temperature is 850 ℃, the applied pressure is 20MPa, the sintering heat preservation time is 5min, and demolding after natural cooling to obtain the oxygen-free copper-based high-strength composite material.
The temperature rise process of spark plasma sintering is as follows: and vacuumizing the sintering furnace chamber to 5Pa, starting heating, heating to 650 ℃ at the speed of 100 ℃/s, preserving the temperature for 5min, and then heating to the sintering temperature of 850 ℃ at the speed of 100 ℃/s.
The preparation method of the graphene/copper composite powder in the first step comprises the following steps:
the method comprises the following steps: adding copper acetate into ammonia water, and uniformly mixing to obtain a copper ammonia solution;
step two: adding graphite oxide sol into the copper ammonia solution obtained in the step one, and carrying out ultrasonic treatment for 40 minutes to obtain a mixed solution A;
the preparation method comprises the following steps of preparing graphite oxide sol, namely dispersing graphene oxide powder in water, and carrying out ultrasonic treatment to obtain graphite oxide sol;
step three: stirring the mixed solution A by a magnetic stirrer for 30 minutes at a speed of 200r/min, heating the mixed solution A to 100 ℃, and evaporating to obtain mixed powder;
step four: continuously heating the mixed powder to 240 ℃, heating for 6-8 hours until the mixed powder is dried to obtain dry powder, and introducing hydrogen into the dry powder to carry out reduction treatment to obtain the graphene/copper composite powder;
wherein the introduction rate of hydrogen is 10 mL/min.
Example 2
A preparation process of an oxygen-free copper-based high-strength composite material comprises the following steps:
the method comprises the following steps: uniformly mixing chromium powder, nano titanium carbide and graphene/copper composite powder according to the formula amount to obtain a mixture;
wherein the mixture comprises the following raw materials in parts by weight: 15 parts of chromium powder, 3 parts of nano titanium carbide and 80 parts of graphene/copper composite powder;
the graphene/copper composite powder comprises copper acetate, ammonia water and graphite oxide sol, wherein the mass ratio of the copper acetate to the ammonia water to the graphite oxide sol is 1:2: 1;
the chromium powder is prepared by ball milling raw material chromium powder with the particle size range of 50-200 mu m and the median particle size of 100 mu m; the nano titanium carbide is prepared by ball milling raw material nano titanium carbide with the particle size range of 100-300 mu m and the median particle size of 120 mu m;
step two: and (3) placing the mixture obtained in the step one in a mould, performing discharge plasma sintering in an argon environment, wherein the sintering temperature is 950 ℃, the applied pressure is 40MPa, the sintering heat preservation time is 6min, and demolding after natural cooling to obtain the oxygen-free copper-based high-strength composite material.
The temperature rise process of spark plasma sintering is as follows: and vacuumizing the sintering furnace chamber to 5Pa, starting heating, keeping the temperature at 650 ℃ at the speed of 100 ℃/s, keeping the temperature for 6min, and then heating to the sintering temperature of 950 ℃ at the speed of 100 ℃/s.
The preparation method of the graphene/copper composite powder in the first step comprises the following steps:
the method comprises the following steps: adding copper acetate into ammonia water, and uniformly mixing to obtain a copper ammonia solution;
step two: adding graphite oxide sol into the copper ammonia solution obtained in the step one, and carrying out ultrasonic treatment for 40 minutes to obtain a mixed solution A;
the preparation method comprises the following steps of preparing graphite oxide sol, namely dispersing graphene oxide powder in water, and carrying out ultrasonic treatment to obtain graphite oxide sol;
step three: stirring the mixed solution A for 30 minutes at a speed of 200r/min by a magnetic stirrer, heating the mixed solution A to 100 ℃, and evaporating to dryness to obtain mixed powder;
step four: continuously heating the mixed powder to 240 ℃, heating for 6-8 hours until the mixed powder is dried to obtain dry powder, and introducing hydrogen into the dry powder to carry out reduction treatment to obtain the graphene/copper composite powder;
wherein the introduction rate of hydrogen is 10 mL/min.
Example 3
A preparation process of an oxygen-free copper-based high-strength composite material comprises the following steps:
the method comprises the following steps: uniformly mixing chromium powder, nano titanium carbide and graphene/copper composite powder according to the formula amount to obtain a mixture;
wherein the mixture comprises the following raw materials in parts by weight: 30 parts of chromium powder, 5 parts of nano titanium carbide and 90 parts of graphene/copper composite powder;
the graphene/copper composite powder comprises copper acetate, ammonia water and graphite oxide sol, wherein the mass ratio of the copper acetate to the ammonia water to the graphite oxide sol is 1:2: 1;
the chromium powder is prepared by ball milling raw material chromium powder with the particle size range of 50-200 mu m and the median particle size of 100 mu m; the nano titanium carbide is prepared by ball milling raw material nano titanium carbide with the particle size range of 100-300 mu m and the median particle size of 120 mu m;
step two: and (3) placing the mixture obtained in the step one in a mould, performing discharge plasma sintering in an argon environment, wherein the sintering temperature is 1000 ℃, the applied pressure is 50MPa, the sintering heat preservation time is 7min, and demolding after natural cooling to obtain the oxygen-free copper-based high-strength composite material.
The temperature rise process of spark plasma sintering is as follows: and vacuumizing the sintering furnace chamber to 5Pa, starting heating, heating to 650 ℃ at the speed of 100 ℃/s, preserving heat for 7min, and then heating to 1000 ℃ at the speed of 100 ℃/s.
The preparation method of the graphene/copper composite powder in the first step comprises the following steps:
the method comprises the following steps: adding copper acetate into ammonia water, and uniformly mixing to obtain a copper ammonia solution;
step two: adding graphite oxide sol into the copper ammonia solution obtained in the step one, and carrying out ultrasonic treatment for 40 minutes to obtain a mixed solution A;
the preparation method comprises the following steps of preparing graphite oxide sol, namely dispersing graphene oxide powder in water, and carrying out ultrasonic treatment to obtain graphite oxide sol;
step three: stirring the mixed solution A for 30 minutes at a speed of 200r/min by a magnetic stirrer, heating the mixed solution A to 100 ℃, and evaporating to dryness to obtain mixed powder;
step four: continuously heating the mixed powder to 240 ℃, heating for 6-8 hours until the mixed powder is dried to obtain dry powder, and introducing hydrogen into the dry powder to carry out reduction treatment to obtain the graphene/copper composite powder;
wherein the introduction rate of hydrogen is 10 mL/min.
Comparative example 1
The copper-based electric contact composite material with the patent number of CN 105220004B and the preparation method thereof are adopted;
comparative example 2
Producing the obtained oxygen-free copper-based high-strength composite material by adopting chromium powder, nano titanium carbide and copper alloy according to the preparation process of the embodiment 1-3;
tensile stress, conductivity and hardness tests were conducted on examples 1 to 3 and comparative examples 1 to 2; the method comprises the following steps of carrying out room-temperature tensile property test on a tensile sample prepared by linear cutting on an AGS-J universal tester, wherein the tensile rate is 0.5mm/min, the tensile width of the tensile sample is 6mm, the tensile length is 15mm, and the thickness of the sample is 2 mm; testing the conductivity of the composite material by using a conductivity meter; testing the hardness of the material by using a high-temperature Vickers hardness tester;
the test results are shown in the following table:
| tensile Strength (GPa) | Electrical conductivity (% IACS) | Hardness (HV) | |
| Example 1 | 2.61 | 82.3 | 152 |
| Example 2 | 2.63 | 82.7 | 154 |
| Example 3 | 2.66 | 83.1 | 155 |
| Comparative example 1 | 2.45 | 70.4 | 151 |
| Comparative example 2 | 1.28 | 69.5 | 121 |
From the above table, it can be seen that the tensile strength of the oxygen-free copper-based high-strength composite material prepared in examples 1-3 is 2.61-2.66GPa, which is much higher than that of the homemade oxygen-free copper-based high-strength composite material of comparative example 2; the conductivity (% IACS) of the oxygen-free copper-based high-strength composite material prepared in examples 1 to 3 was 82.3 to 83.1, which is much higher than that of comparative examples 1 to 2; the hardness of the oxygen-free copper-based high-strength composite material (HV) prepared in examples 1-3 is 152-155, which is much higher than that of the self-made oxygen-free copper-based high-strength composite material prepared in comparative example 2;
therefore, the oxygen-free copper-based high-strength composite material prepared by the invention has excellent strength and conductivity.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (10)
1. The preparation process of the oxygen-free copper-based high-strength composite material is characterized by comprising the following steps of:
the method comprises the following steps: uniformly mixing chromium powder, nano titanium carbide and graphene/copper composite powder according to the formula amount to obtain a mixture;
step two: and (3) placing the mixture obtained in the step one in a mold, performing discharge plasma sintering under protective gas, wherein the sintering temperature is 850-1000 ℃, the applied pressure is 20-50MPa, the sintering heat preservation time is 5-7min, and demolding after natural cooling to obtain the oxygen-free copper-based high-strength composite material.
2. The preparation process of the oxygen-free copper-based high-strength composite material as claimed in claim 1, wherein the preparation of the graphene/copper composite powder in the first step comprises the following steps:
s1: adding copper acetate into ammonia water, and uniformly mixing to obtain a copper ammonia solution;
s2: adding graphite oxide sol into the copper ammonia solution obtained in the step S2, and carrying out ultrasonic treatment for 35-45 minutes to obtain a mixed solution A;
s3: stirring the mixed solution A for 30 minutes at a speed of 200r/min by a magnetic stirrer, heating the mixed solution A to 100 ℃, and evaporating to dryness to obtain mixed powder;
s4: and heating the mixed powder until the mixed powder is dried to obtain dry powder, and reducing the dry powder to obtain the graphene/copper composite powder.
3. The preparation process of the oxygen-free copper-based high-strength composite material as claimed in claim 2, wherein the mass ratio of the copper acetate, the ammonia water and the graphite oxide sol is 1:2: 1.
4. The preparation process of the oxygen-free copper-based high-strength composite material as claimed in claim 2, wherein the preparation of the graphite oxide sol is to disperse graphene oxide powder in water and obtain the graphite oxide sol by ultrasonic treatment.
5. The preparation process of the oxygen-free copper-based high-strength composite material as claimed in claim 2, wherein the heating temperature of the mixed powder in the S4 is 240 ℃, and the continuous heating time is 6-8 hours.
6. The preparation process of the oxygen-free copper-based high-strength composite material as claimed in claim 2, wherein the dry powder is subjected to reduction treatment by hydrogen in S4, and the introduction rate of the hydrogen is 10 mL/min.
7. The preparation process of the oxygen-free copper-based high-strength composite material as claimed in claim 1, wherein the weight ratio of the chromium powder, the nano titanium carbide and the graphene/copper composite powder is 10-30: 1-5: 70-90.
8. The preparation process of the oxygen-free copper-based high-strength composite material as claimed in claim 1, wherein the chromium powder is prepared by ball milling of raw material chromium powder with a particle size range of 50-200 μm and a median particle size of 100 μm;
the nano titanium carbide is prepared by ball milling raw material nano titanium carbide with the particle size range of 100-300 mu m and the median particle size of 120 mu m.
9. The process for preparing an oxygen-free copper-based high-strength composite material as claimed in claim 1, wherein the protective gas in the second step is argon.
10. The process for preparing the oxygen-free copper-based high-strength composite material according to claim 1, wherein the temperature rise process of the spark plasma sintering in the second step is as follows: the sintering furnace chamber is vacuumized to 5Pa and then heated to 650 ℃ at the speed of 100 ℃/s, and after the temperature is kept for 5-7min, the temperature is raised to the sintering temperature of 850 ℃ and 1000 ℃ at the speed of 100 ℃/s.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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